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Optical Materials 35 (2013) 11291133

Contents lists available at SciVerse ScienceDirect

Optical Materials
journal homepage: www.elsevier.com/locate/optmat

Thermal mirror spectrometry: An experimental investigation of optical glasses

V.S. Zanuto a, L.S. Herculano a, M.L. Baesso a, G.V.B. Lukasievicz a,b, C. Jacinto c, L.C. Malacarne a,
N.G.C. Astrath a,
a

Departamento de Fsica, Universidade Estadual de Maring, Maring, PR 87020-900, Brazil

CAPES Foundation, Ministry of Education of Brazil, Braslia, DF 70040-020, Brazil
c
Instituto de Fsica, Universidade Federal de Alagoas, Macei, AL 57072-970, Brazil
b

a r t i c l e

i n f o

Article history:
Received 31 October 2012
Received in revised form 31 December 2012
Accepted 2 January 2013
Available online 8 February 2013
Keywords:
Thermal mirror
Thermo-optical properties
Optical materials

a b s t r a c t
The Thermal mirror technique relies on measuring laser-induced nanoscale surface deformation of a solid
sample. The amplitude of the effect is directly dependent on the optical absorption and linear thermal
expansion coefcients, and the time evolution depends on the heat diffusion properties of the sample.
Measurement of transient signals provide direct access to thermal, optical and mechanical properties
of the material. The theoretical models describing this effect can be formulated for very low optical
absorbing and for absorbing materials. In addition, the theories describing the effect apply for semi-innite and nite samples. In this work, we apply the Thermal mirror technique to measure physical properties of optical glasses. The semi-innite and nite models are used to investigate very low optical
absorbing glasses. The thickness limit for which the semi-innite model retrieves the correct values of
the thermal diffusivity and amplitude of the transient is obtained using the nite description. This procedure is also employed on absorbing glasses, and the semi-innite BeerLambert law model is used to
analyze the experimental data. The experimental data show the need to use the nite model for samples
with very low bulk absorption coefcients and thicknesses L < 1.5 mm. This analysis helped to establish
limit values of thickness for which the semi-innite model for absorbing materials could be used,
L > 1.0 mm in this case. In addition, the physical properties of the samples were calculated and absolute
values derived.
2013 Elsevier B.V. All rights reserved.

1. Introduction
Laser induced surface deformation has been explored in many
photothermal (PT) techniques [14]. These techniques are characterized as fast, non-contacting and highly sensitive spectroscopic
tools for material characterization. The reason is that there are
many different experimental congurations that are important in
many research aspects, such as nondestructive evaluation of solids
and surfaces, from multilayered and thin lms to biological systems [513]. The amplitude of the deformation is directly related
to the optical absorption and linear thermal expansion coefcients,
and the time evolution of the deformation depends on the heat diffusion properties. Thus, measuring the transient effect implies direct quantitate access to thermal, optical and mechanical
properties of the material [1016].
Surface deformation can be generated by modulated [511] or
pulsed [1214] excitation lasers. Briey, the principle of detection
of these PT methods consists of measuring the surface displacement of the sample by pumpprobe methods. For instance, this
deformation can be detected by analyzing the focusing/defocusing
Corresponding author.
E-mail address: astrathngc@pq.cnpq.br (N.G.C. Astrath).
0925-3467/$ - see front matter 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.optmat.2013.01.003

of the probe beam reected off of the sample surface in the far eld
region. In this conguration, namely Thermal Mirror (TM) spectrometry, the method has been recently introduced under cw
Gaussian [1518] and Top-hat [19,20] laser excitations for measurement of thermal diffusivity and thermo-optical properties of
semi-transparent and opaque solids. TM is attractive in that it
can also be used concurrently with the Thermal Lens method to
determine physical properties of uorescent materials [19].
Recent theoretical and experimental works for Gaussian excitation have been developed assuming the sample either as a semiinnite [17] or as a nite [18] media. Under the semi-innite
approximation, the sample is treated as an innite medium along
the z axis with its surface placed at z = 0. For the nite approach,
the sample surfaces are at z = 0,L. The thermoelastic equations
describing the laser induced surface displacement were solved
according to these assumptions and experimental investigations
of very low bulk absorbing materials were compared to the theories. It was shown that for samples with thicknesses under certain
values the nite model should be considered. However, the nite
description allows only solutions for materials with low optical
absorption coefcient (Ae), where the attenuation of light intensity
is considerably negligible along the sample thickness. For absorbing samples, in which the light intensity attenuation follows the

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V.S. Zanuto et al. / Optical Materials 35 (2013) 11291133

BeerLambert law as eAe z , only semi-innite solutions for the thermoelastic equations are semi-analytically available. Here, we further investigate the nite and semi-innite approaches by
performing experiments in very transparent and absorbing optical
glasses.
In this work, we apply the Thermal mirror technique to measure
physical properties of optical glasses. These glasses have optical
absorption coefcients varying from approximately 61150 m1.
The semi-innite and nite models are used to investigate the
low optical absorbing glasses (Ae < 200 m1). The thickness limit
for which the semi-innite model retrieves the correct values of
the thermal diffusivity and TM amplitude is obtained using the nite description. This procedure is also employed on absorbing
glasses, and the semi-innite BeerLambert law model is used to
analyze the experimental data for Ae > 400 m1.
2. Theory
The TM experiment was performed in the dual beam modemismatched conguration, as shown in Fig. 1. In this conguration,
the sample is excited and probed by single-mode TEM00 Gaussian
cw laser beams with radii x0e and x1p (on the sample surface at
z = 0), respectively [17]. The excitation laser beam induces a nonuniform temperature gradient deforming the sample surface
accordingly. The probe beam is reected off of the sample surface
and senses the deformation along the z-axis. The amplitude of the
TM effect is directly related to the absorption coefcient and surface bulging, and the time evolution of the deformation depends
on the heat diffusion properties. The deformation evolves following the NavierStokes thermoelastic equation [21]. Due to the axially symmetric radial nature of the Gaussian heat source, the
problem is treated in cylindrical coordinates and, in the quasi-static approximation, the solution is proposed by introducing the scalar displacement potential W and the Love function was described
in details in Ref. [21]. Using the integral transform method it is
possible to write the surface displacement, uz(r,z = 0,t), as [18]

uz r; 0; t 2aT 1 m

r Z
2

a2 Ta; k; t  a2

k2 1 ha; kJ0 a r dk da;

where aT is the linear thermal expansion coefcient, m is the Poissons ratio and Jn(x) represents the Bessel function of the rst kind.
T(a,k,t) is the temperature in the HankelFourier space and h(a,k),
for a nite sample of thickness L, is given by [18]

ha; k

1
2

1 2L a  cosh2La
2

 f2La sinh2La

 2Lk sinhLa sinLk  2La coshLa sinhLa

 cosLkg:

For a semi-innite sample, h(a,k) = 1 [15]. Eq. (1) does not consider
sample-uid heat coupling this assumption has been investigated
in Ref. [22] and was found to be a good approximation when air is
used as uid. Assuming that the radial dimensions of the sample are
much larger than the radii of probe and excitation beams on the
sample; the solution of the heat diffusion equation can be calculated for a material whose absorption of light follows the BeerLambert law (BLM) yielding [16]

Ta; k; t

x2 a2
P e Ae /
0e
Qke 8
2pqc

2 k2

eDa

ds:


p 
Q k Ae 2=p= A2e k2 is the FourierCosine transform of the
azimuthal source term Sz eAe z . S(z) accounts for the attenuation
of light along the sample thickness. In the limit of very low bulk
absorption coefcient, Low
Model (LAM), Ae ? 0 and

pAbsorption
S(z) = 1, yielding Q k 2pdk. d(k) represents the Dirac delta
function. Pe = P0(1  R), P0 is the excitation power, R is the sample
surface reectivity, / measures the fraction of the absorbed energy
converted to heat, ke is the excitation beam wavelength. D, q and c
are the thermal diffusivity, mass density and the specic heat of the
sample, respectively.
The general BLM representation of the displacement can be
semi-analytically calculated only for the semi-innite approximation. On the other hand, the approximate LAM presents solutions
for both nite and semi-innite descriptions.
The temperature rise distribution induces a surface displacement that acts as an optical element, causing a phase shift of the
probe beam reected off of the sample surface as U(r,t) = (2p/
kp)2[uz(r,0,t)  uz(0, 0, t)] [17]. kp is the probe beam wavelength.
By introducing the characteristic TM thermal time t c x20e =4D,
and using Eq. (1), the phase shift for the semi-innite BLM can
be written as [16]

USIBLM g; t

hTM

tc

1 2

a2 e8a x0e f a; tJ0 ax0e gm  1da; 4

in which

 2 2 
p

p
a x t
x0e
2 tc t Ae x0e exp  4tc0e
t Ae x20e Erfc t2ap
tc
f a; t

p 4
pa  a2 A2e
a3  aA2e
p





2tc
tax0e
p

A3e  3a2 Ae Erf
2 
2 tc
a3 a2  A2e

2 2
3
2
39
p
 =
Ae  a2 x20e
t
A
x
e
0e
5  Erfc
5 :
p
2 a3 41  exp 4
;
4t c =t
2 tc

For the nite LAM [18],

x20e

coshLa  1
La sinhLa
Z t x2
p
2s
2
0e
 J0 ax0e gm  1
e 8 1 tc a ds da;

UFLAM g; t hTM

tc

and for the semi-innite LAM [15,17],

Fig. 1. Schematic diagram of an apparatus for time-resolved TM experiment. Li, Mi,
Pi and f stand for lenses, mirrors, photodiodes and focal distances, respectively.

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V.S. Zanuto et al. / Optical Materials 35 (2013) 11291133

USILAM g; t hTM

x20e
tc

x2

e

0e
8

12tcsa2 ds

p
 J0 ax0e gm  1da:

Here, the parameter hTM measures the amplitude of the TM effect and is given by

hTM 

P e Ae aT 1 m/
;
kp k

with k representing the thermal conductivity of the sample. g = (r/

x1p)2 and m = (x1p/x0e)2. Note that the semi-innite approximation can be obtained from Eq. (6) taking the limit L ? 1.
The propagation of a TEM00 Gaussian reected probe beam can
be treated using Fresnel diffraction theory. Considering only the
center point of the probe beam at the detector plane its intensity
is given by [17]

2
R 1

iVg  i Ug; t dg 
 0 exp1
R1
It I0
 :


exp1 iVg dg
0

V = Z1/ZC + ZC[(Z1/ZC)2 + 1]/Z2. Z1 is the distance from the probe

beam waist (with radius x0p) to the sample, ZC is the confocal distance of the probe beam, Z2 is the distance from the sample to the
sensor plane, and I(0) is the intensity at t = 0. I(t) is calculated by
substituting one of the equations for the phase shift, Eqs. (4), (6)
or (7), into Eq. (9) and carrying out numerical integration over a,
s and g.
The temperature changes are generally small in these TM
experiments, <1 K. The index change induced by surface heating
is similarly small. Subsequently, changes in the probe beam intensity due to surface reectivity effects can be safely neglected without affecting the accuracy of the results.
The optical absorption range in which the LAM and BLM models
could be used has been tested theoretically [17,18] and it was veried that for Ae < 200 m1 the LAM approximation represents quite
well the BLM complete model.
3. Experimental
A schematic diagram of the experimental apparatus for TM
measurement is presented in Fig. 1. The excitation source is a cw
single-mode TEM00 Ar+ ion laser at ke = 514.5 nm (Coherent, Innova
90). A mechanical shutter (ThorLabs, Model SH05) controls the
exposure of the excitation beam power on the sample. The excitation beam was focused on the sample surface using a 25 cm focal
length lens. Either a continuous TEM00 Gaussian HeNe laser at
kp = 632.8 nm (Melles Griot, Model 25-LHR-151-249) or a Ti:Sapphire laser at kp = 976 nm (Spectra-Physics, Model 3900S), almost
collinear to the excitation beam (c < 1.0), are used to probe the
TM. After being reected off of the sample surface, the probe beam
propagates to the photodetector (P1) positioned in a far eld
(Z2 > 4 m). P1 (ThorLabs, Model DET100A/M) was assembled with
a pinhole and a probe beam laser line lter. Only the central part
of the probe beam is detected by the photodiode and recorded
by a digital oscilloscope (Tektronix, Model TDS 1001B). The oscilloscope is triggered by P2 (ThorLabs, Model PDA10A).
Table 1
Physical properties of the samples

D
hTM/Pe

aT
Ae

qc

During the TM measurement, the intensity at the center of the

probe beam is monitored as a function of time. This transient signal
is then transferred to a computer and the theoretical model is subsequently tted to the data providing information regarding the
properties of the sample. tc and hTM are retrieved from the ts. tc
is related to the thermal diffusivity and hTM to the thermo-optical-mechanical properties of the sample.
Complementary measurements of linear thermal expansion
coefcient, specic heat and mass density, all at room temperature
were performed using a commercial horizontal pushrod dilatometer (NETZSCH DIL 402 PC), a homemade thermal relaxation calorimeter and a standard Archimedes method, respectively. The
dimensions of the samples for the dilatometer were
15  3  3 mm. A laser beam was used as the heat source for the
calorimeter, as described in Ref. [23]. The samples used in these
measurements were 1 mm thick with about 30 mg, the condition
in which the internal relaxation time is negligible.
To test the nite and semi-innite models and show the applicability of the technique in the study of transparent and absorbing
materials, we performed measurements of low-silica-calcium-aluminosilicate (LSCAS), soda-lime (SL) and phosphate glasses. The
compositions of the samples are, in wt.%, 47.4 CaO(41.5  x  y)
Al2O37.0 SiO24.1 MgO x CeO2y Cr2O3, with x = 2 and y = 0
(LSCAS-Ce), and with x = 0 and y = 0.5 (LSCAS-Cr), 68.4 SiO217.6
Na2O10 CaO4 MnO2 (SLMn), and two phosphate samples doped
with 5 wt.% Yb2O3 (QX), and 1 wt.% Nd2O3 (Q98), both manufactured by Kigre Inc. The samples are approximately 1 cm in diameter and with thicknesses within the range of 0.426.10 mm. The
samples were optically polished to present highly reective surfaces. The optical absorption coefcients of samples were determined by measuring the incident and transmitted powers, for
the several different thicknesses, at the excitation wavelength.
The values are presented in Table 1. Optical reection coefcients
were determined from refractive index data (Ref. [24] for LSCAS
and SL, and measured using an Abbe Refractometer NAR-4T for
QX and Q98). Poissons ratio are available in Ref. [24] for LSCAS
and SL, and from vendors for QX and Q98.
The experimental parameters, x1p and x0e, for the excitation
and probe beams were determined by measuring the excitation
and probe beam radii at different positions z with a beam proler
(ThorLabs, Model BP104-UV), and used to determine the confocal
distance Z C px20p =kp and Z1. Different experimental congurations were used in this work and the experimental parameters
are displayed in the following gures.
4. Results and discussion
The TM measurements were performed at room temperature.
The samples were excited for 450 ms, in different excitation powers, varying from 0.03 to 2 W. Fig. 2 shows examples of normalized
TM transients for the QX samples with different thicknesses under
the excitation power of P0 = 0.82 W. The inuence of the thickness
over the TM amplitude can clearly be seen. As the thickness is reduced, the transient amplitude diminishes accordingly. TM transients were tted to the semi-innite (dashed lines) and nite
(continuous lines) LAM models. Note that both the semi-innite
and nite approximations are in excellent agreement with the

Ref. [25].

107 m2s1
m1 W1
107 K1
m1
106JK1 m3

QX

Q98

LSCAS-Ce

SLMn

LSCAS-Cr

3.6 0.3
114 3
83a
6.03 0.05
1.97 0.05

2.8 0.2
746 43
99 5
48.5 0.7
2.48a

5.4 0.4
85 3
76 4
7.5 0.9
2.42 0.08

7.3 0.3
(3.4 0.1)  103
90 4
460 18
1.98 0.05

7.1 0.3
(7.8 0.4)  103
89 4
1158 30
2.40 0.05

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V.S. Zanuto et al. / Optical Materials 35 (2013) 11291133

(a)

(b)

Fig. 2. Normalized Thermal mirror signal I(t)/I(0) for the QX samples of different
thicknesses under excitation of P0 = 0.82 W. Circle: experimental data; dashed line:
best curve tting using the semi-innite LAM model; solid line: best curve tting
using the nite LAM model. The experimental parameters are Z1 = 8.8 cm, ZC =
1.31 cm, x0e = 71 lm, x1p = 360 lm, m = 25.7, and V = 6.71.

Fig. 4. Experimental results for the phosphate Q98 and LSCAS-Ce glasses: (a) shows
the thermal diffusivities and (b) the parameter hTM/P e obtained from tting to the
nite, Eq. (6), and semi-innite, Eq. (7), models for different thicknesses. The
experimental parameters are Z1 = 8.3 cm, ZC = 1.47 cm, x0e = 104 lm, x1p = 316 lm,
m = 9.14, and V = 5.6 for Q98, and Z1 = 15.8 cm, ZC = 2 cm, x0e = 72 lm,
x1p = 501 lm, m = 48.5, and V = 7.9 for LSCAS-Ce.

(a)

(a)

(b)

(b)

Fig. 3. Experimental results for the phosphate QX glass: (a) shows the thermal
diffusivities and (b) the parameter hTM/Pe obtained from tting to the nite, Eq. (6),
and semi-innite, Eq. (7), models for different thicknesses.

experimental data for the thicker sample while for L = 0.42 mm the
semi-innite model does not t well to the data.
The thermal diffusivities and the parameters hTM obtained from
the regressions are shown in Fig. 3. Both models retrieve approximately the same values as the thickness is increased, although the
semi-innite model over predicts the thermal diffusivity and the
parameter hTM as the thickness is reduced. Note that the thick sample falls into the semi-innite approximation; hTM and D are
approximately the same as the ones obtained using the nite model. The gray areas show the region within the acceptable values for
D and hTM from the nite analises, and the average parameters are
presented in Table 1.
The same behavior is also observed for Q98 and LSCAS-Ce
glasses. Fig. 4 shows the thermal diffusivity and the parameter
hTM/Pe for different thicknesses of the samples. It is evident that
as the thickness is reduced to values lower than L = 1.5 mm the
semi-innite approximation cannot be used to analyze the experimental data. In fact, it does not pose major problems because of
low optical absorption materials the nite modeling is available.
However, for materials not following the LAM approximation only

Fig. 5. Experimental results for LSCAS-Cr and SLMn glasses: (a) shows the thermal
diffusivities and (b) the parameter hTM/Pe obtained from tting to the semi-innite
BLM model, Eq. (4), for different thicknesses. Dashed and dotted lines show the
average parameters obtained from the thick samples. The experimental parameters
for both samples are Z1 = 5.75 cm, ZC = 6.4 cm, x0e = 80 lm, x1p = 200 lm, m = 6.25,
and V = 0.89.

a semi-innite description is possible and the thickness of the sample has to be chosen according to the modeling approximation.
Fig. 5 displays the results for the soda-lime and LSCAS-Cr samples with different thicknesses. D and hTM/Pe were obtained from
the experimental transients tted to I(t) with Eq. (4). Dashed and
dotted lines show the average parameters obtained from the thick
samples. The averaged values are also presented in Table 1. It can
be seen that even for samples with thickness around L = 1 mm the
semi-innite approximation gives values of D and hTM/Pe close to
the ones of the thicker samples. This lower thickness limit of validity of the semi-innite BLM model compared to the semi-innite
LAM can be explained by the fact that in samples with high optical
absorption coefcient, the contribution to the TM phase shift is
mainly supercial. The attenuation of light along the sample thickness makes the inner layers to contribute less to the deformation
prole. The same does not happen for very low optical absorbing
materials, where the sample absorbs practically evenly within
the material.

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V.S. Zanuto et al. / Optical Materials 35 (2013) 11291133

With the additional values of qc and aT (presented in Table 1)

and the parameters hTM/Pe and k = qc D obtained from the TM measurements, / can be calculated. /  1 was obtained for QX, LSCASCe, LSCAS-Cr and SLMn glasses. This means that all the absorbed
energy was converted into heat. This is the case for samples with
no uorescence under the excitation wavelength. In other words,
if one compare the measured values of hTM/Pe for these samples
with the calculated ones using the right hand side of Eq. (8), the results are in excellent agreement. For the Q98, ke = 514.5 nm excites
the 4F3/2 Nd3+ energy level. For this sample, / = 0.54 0.03, and it
can be evaluated by / = 1  g ke/hkemi, in which ke is the excitation
beam wavelength, hkemi is the mean emission wavelength, and g is
the uorescence quantum efciency. Using hkemi = 1064 nm [25],
g = 0.95 0.06 was calculated. This is in excellent agreement with
previous measurements [25].
It is important to mention that for very low optical absorption
materials, the semi-innite approximation can be used for samples
with thickness L > 1.5 mm. The only advantage of using this
approximation is that the numerical tting routines are much faster than the nite ones. On the other hand, the nite model is available and can be used whenever thin samples are to be investigated.
The comparison between semi-innite and nite LAM models are
important to establish a background for using the BLM model.
For BLM, only semi-innite approximation can be computed. The
results presented here provide information regarding the thickness
limits in which the semi-innite approximation could be used.
5. Conclusion
In conclusion, we used the Thermal mirror technique and the
theoretical models considering the sample as a nite or semi-innite media to investigate thermal, optical and mechanical properties of optical glasses. The experimental data show the need to use
the nite model for the analysis of samples of very low bulk
absorption coefcients and with thicknesses L < 1.5 mm. The
semi-innite and nite investigation helped to establish limit values of thickness for which the semi-innite model for absorbing
materials could be used, L > 1.0 mm in this case. In addition, the
physical properties of the samples were calculated and absolute
values derived.
Acknowledgements
The authors are thankful to the Brazilian Agencies CAPES (Coor vel Superior), CNPq
denao de Aperfeioamento de Pessoal de N
(Conselho Nacional de Desenvolvimento Cientco e Tecnolgico),
and Fundao Araucria for the nancial support of this work.
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